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실시간 In-situ IR을 이용한 Glycidyl Azide Monomer(GAM)의 양이온중합 반응속도 연구
김형석,김관영,강신춘,노시태,김진석,유재철,최근배,Kim, Hyoung-Sug,Kim, Kwan-Yung,Kang, Shin-Choon,Noh, Si-Tae,Kim, Jin-Seuk,Yu, Jae-Chul,Choi, Keun-Bae 한국군사과학기술학회 2009 한국군사과학기술학회지 Vol.12 No.2
We synthesized glycidyl azide monomer(GAM) as a monomer for polymerization of glycidy azide polymer(GAP) which is a promising energetic prepolymer for a plastic-bonded explosive. Using quantitative real-tim in-situ infrared(in-situ IR) spectroscopy, kinetic study on the cationic ring opening polymerization of GAM was carried out. The reaction rate was obtained from monitoring the change of ether C-O stretching band($1050cm^{-1}$) in series IR spectra. The reaction was in accordance with the first-order reaction law for each of reaction temperature at 100/1 mole ratio of [GAM]/[$BF_3*etherate$]. In the ring opening polymerization of GAM, with ratio of [GAM]/[$BF_3*etherate$] to equal 100/1 at various temperature, the activation parameters obtained from the evaluation of kinetic data were ${\Delta}H^*$=14.34kcal/mol, ${\Delta}S^*=-12.31cal/mol{\cdot}K$ and $E_a$=14.89kcal/mol.
실시간 In-situ IR을 사용한 벌크상 Poly(oxytetramethylene) Glycol과 Isophorone Diisocyanate의 반응속도론 연구
김정균 ( Jung Kyun Kim ),조항규 ( Hang Kyu Cho ),노시태 ( Si Tae Noh ),강신춘 ( Shin Choon Kang ) 한국공업화학회 2002 공업화학 Vol.13 No.8
실시간 정량적 분석이 가능한 In-situ IR을 사용하여 poly(oxytetramethylene) glycol (PTMG)과 isophoron diisocyanate(IPDI) 간의 반응 속도론적 연구를 수행하였다. 반응 속도는 일련의 IR 스펙트럼에서 NCO 신축진동흡수(2265 cm^1) 및 C=O 신축진동흡수(1725 cm^1)대의 흡광도 변화를 모니터링하여 얻었다. 반응은 수산기와 이소시아네이트기의 농도에 대하여 각각 1차이고, 전체적으로 2차인 반응 속도법칙에 따랐다. PTMG와 IPDI의 벌크 중합에서 [NCOJ/[OH]=1.0일 때 반응 속도 상수로부터 구한 활성화 파라미터는 E_a = 61.07 kJ/mol, △H^* = 58.18 kJ/mol 및 △S^# = -95.98 J/molㆍK 이었다. Using quantitative real-time In-situ infrared (In-situ IR) spectroscopy, kinetic study of a reaction between isophoron diisocyanate (IPDI) and poly(oxytetramethylene) glycol (PTMG) was carried out. The reaction rate was obtained from monitoring the change of NCO (2265 cm^-1) and C=O (1725 cm^-1) stretching band in series IR spectra. The reaction was in accordance with the first-order reaction for each concentration of hydroxyl groups and isocyanate group, respectively, however, the overall reaction conformed to the second-order law. In the bulk polymerization between PTMG and IPDI, with ratio of [NCOJ/[OH] equal to 1.0 at various temperatures, the activation parameters obtained from the evaluation of kinetic data were △H^* = 58.18 kJ/mol, △S^# = -95.98 J/molㆍK and E_a = 61.07 kJ/mol.